反应 #586134

反应方程式

water

2-chloro-4-(4-trifluoromethylpyrazolyl)benzonitrile

2,2,2-trifluoroethanthiol

potassium carbonate

→

2-(2,2,2-trifluoroethylthio)-4-(4-trifluoromethylpyrazolyl)benzonitrile

收率 57.1%

溶剂

N,N-dimethylformamide

反应条件

后处理

1. 1
   其他The resulting reaction mixture
2. 2
   萃取the organic matters were extracted with 20 ml of ethyl acetate twice
3. 3
   洗涤washed with 30 ml of water twice
4. 4
   干燥dried over anhydrous magnesium sulfate
5. 5
   workup.DISTILLATIONthe ethyl acetate was distilled off under reduced pressure
6. 6
   其他Purification of the residue by silica gel column chromatography

实验过程

0.65 g (2.4 mmol) of 2-chloro-4-(4-trifluoromethylpyrazolyl)benzonitrile, 0.33 g (2.9 mmol) of 2,2,2-trifluoroethanthiol and 0.40 g (2.9 mmol) of potassium carbonate were stirred in 5 ml of N,N-dimethylformamide at room temperature overnight. The resulting reaction mixture was poured into 50 ml of water, and the organic matters were extracted with 20 ml of ethyl acetate twice. The ethyl acetate layers were combined, washed with 30 ml of water twice and dried over anhydrous magnesium sulfate, and the ethyl acetate was distilled off under reduced pressure. Purification of the residue by silica gel column chromatography afforded 0.48 g of 2-(2,2,2-trifluoroethylthio)-4-(4-trifluoromethylpyrazolyl)benzonitrile (yield 57.1%) as a milk-white powder (m.p. 90-91° C.).

来源